CN108794938A - Fluorubber, preparation method and the fluorubber rubber roller of primary low-temperature vulcanization - Google Patents
Fluorubber, preparation method and the fluorubber rubber roller of primary low-temperature vulcanization Download PDFInfo
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- CN108794938A CN108794938A CN201810500952.8A CN201810500952A CN108794938A CN 108794938 A CN108794938 A CN 108794938A CN 201810500952 A CN201810500952 A CN 201810500952A CN 108794938 A CN108794938 A CN 108794938A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K5/13—Phenols; Phenolates
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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Abstract
The purpose of the present invention is to solve the energy consumption of fluorubber technique in the prior art, time-consuming problems, provide a kind of fluorubber, preparation method and the fluorubber rubber roller of primary low-temperature vulcanization, belong to polymeric material field.The fluorubber of the present invention is grouped as by the group of following mass fraction ratio:100 parts of crude fluororubber, 12 ~ 18 parts of magnesia, 6 ~ 10 parts of 1,4-butanediol, 35 ~ 45 parts of spray carbon black, 8 ~ 12 parts of ethyl acetate, 0.8 ~ 1.2 part of anti-aging agent RD, 1.5 ~ 2.5 parts of bisphenol-A.Fluororubber formula through the invention, which can be realized, vulcanizes fluorubber primary low-temperature, while still keeping the performance of fluorubber.The preparation method reduces the energy consumption of conventional vulcanizable fluororubber technique, has saved cost.Fluorubber rubber roller product property indices prepared by the formula are better than the product of universal vulcanizing system.
Description
Technical field
The invention belongs to polymeric material fields, more particularly to fluorubber, preparation method and the profit of primary low-temperature vulcanization
The rubber roller prepared with the fluorubber.
Background technology
Fluorubber(fluororubber)It refer to the synthesis high score bullet containing fluorine atom on the carbon atom of main chain or side chain
Property body.The introducing of fluorine atom assigns rubber excellent heat resistance, inoxidizability, oil resistivity, corrosion resistance and resistance to atmospheric aging
Property, it is widely applied in fields such as space flight, aviation, automobile, oil and household electrical appliance, can not be replaced in national defence sophisticated industry
The critical material in generation.
Vulcanization Process of Rubber is mainly that the crosslinked process that chemical reaction is formed occurs for macromolecular chain.Currently, common fluorine
Rubber formula is required to post vulcanization.Post-cure is the steps necessary in its article manufacturing process.Carry out post-cure
Main purpose be:1)Remaining unreacted crosslinked group after once vulcanizing is set to complete reaction;2)It removes and is generated in primary vulcanization
Cross-linking reaction residue, mainly remove in fluorubber product the water that retains and carbon dioxide and a small amount of fluoride or
The fragment etc. that vulcanizing agent generates.Post-cure can improve the mechanical property and compression set performance of product, reduce product
The gas generated during use, and lower the shrinking percentage of product.Therefore, post-cure has emphatically during vulcanizable fluororubber
The effect wanted.
150 DEG C of vulcanizations can also be used generally at 160 ~ 180 DEG C in primary vulcanization, and post-cure is temperature-gradient method to 250 DEG C of sulphur
Change or is vulcanized using 230 DEG C of constant temperature.Therefore, it consumes energy in fluorubber production process and the time is more.
Invention content
The purpose of the present invention is to solve the energy consumption of fluorubber technique in the prior art, time-consuming problems, provide one kind
Fluorubber, preparation method and the fluorubber rubber roller of primary low-temperature vulcanization.Fluororubber formula through the invention can be realized pair
Fluorubber primary low-temperature vulcanizes, while still keeping the performance of fluorubber.The preparation method reduces conventional vulcanizable fluororubber
The energy consumption of technique, has saved cost.Fluorubber rubber roller product property indices prepared by the formula are better than universal vulcanization body
The product of system.
One of technical scheme of the present invention is a kind of fluorubber of primary low-temperature vulcanization, by following mass fraction ratio
Group be grouped as:
100 parts of crude fluororubber
12 ~ 18 parts of magnesia
6 ~ 10 parts of 1,4- butanediols
35 ~ 45 parts of spray carbon black
8 ~ 12 parts of ethyl acetate
0.8 ~ 1.2 part of anti-aging agent RD
1.5 ~ 2.5 parts of bisphenol-A,
Wherein, the Mooney viscosity of the crude fluororubber is 50 ~ 60.
Ethyl acetate in above-mentioned formula plays plasticization in sizing material, instead of softening agent.Use ethyl acetate
Sizing material semi-finished product glue soft texture, the adhesive tape that processing performance well squeezes out is smooth, and can also be reused after secondary operation makes production
Product lumber recovery increases.And ethyl acetate can also play processing aid in sizing material, keep rubber compound easy to process, and
And make the rubber roller product after vulcanization that there is higher elasticity.
1,4-butanediol in above-mentioned formula plays transient plasticizer in process, and joins in sulfidation
With sulfuration effect, it can assign vulcanizate higher crosslink density.Therefore the processing of fluorubber is not only improved using 1,4- butanediols
The quality of performance and product, while also reducing or substituting other materials, such as:The usage amount of softening agent, accelerating agent and carbon black, in this way
Just cost is reduced in the use of raw material.
The two of technical scheme of the present invention are the preparation method of the fluorubber of above-mentioned primary low-temperature vulcanization, including as follows
Step:
1)Bulk portion in the fluorubber each component of primary low-temperature vulcanization is broken into powder;
2)Mixer is warming up to 110 ~ 130 DEG C, is put into crude fluororubber, magnesia, the spray of 1,4-butanediol and 1/2 formula part
Mist carbon black mixes 5 ~ 10 minutes;Remaining material is put into after mixer mixes 4 ~ 6 minutes again and obtains sizing material;
3)Sizing material is put into vulcanizing tank, starts vulcanization reaction after vulcanizing tank is forced into 0.4 ~ 0.6MPa;
The process of vulcanization reaction is:
Vulcanizing tank temperature is set to rise to 100 ~ 110 DEG C in 2 ~ 2.5 hours, after heat preservation vulcanization 1 ~ 1.5 hour, then by vulcanizing tank temperature
120 ~ 135 DEG C, after heat preservation vulcanizes 1.5 ~ 2 hours are risen to, then vulcanizing tank temperature is risen to 140 ~ 155 DEG C, heat preservation vulcanization 8 ~ 10 is small
When after stop heating;Vulcanizing tank is restored to normal pressure, Temperature fall is to 50 DEG C and hereinafter, obtains product.
On inspection, the fluorubber tensile strength 16-18MPa after above method vulcanization, tearing strength 35-45KN/M are pulled apart
Elongation 300-400%, shore hardness 70-75HA wear away 0.210 ~ 0.257cm3/1.6km。
The three of technical scheme of the present invention are a kind of fluorubber rubber roller, by steel roll body and outside the roll body
Above-mentioned primary low-temperature vulcanised fluororubbers crust composition.
The preparation method of above-mentioned fluorubber rubber roller includes the following steps:
1)Bulk portion in the fluorubber each component of primary low-temperature vulcanization is broken into powder;
2)Mixer is warming up to 110 ~ 130 DEG C, is put into crude fluororubber, magnesia, the spray of 1,4-butanediol and 1/2 formula part
Mist carbon black mixes 5 ~ 10 minutes;Remaining material is put into after mixer mixes 4 ~ 6 minutes again and obtains sizing material;
3)Sizing material is subjected to thin logical processing, is pressed into 0.3 ~ 0.7 millimeter of thin slice, then break into triangle bag, repetition 3 ~ 5 times, then
It is pressed into 5-6 millimeters of film on a mill, room temperature is down in ventilation, obtains fluorubber film;
4)In steel roller body surface face brushing adhesive, and film is processed into adhesive tape, system is served as a contrast in roll body with extrusion or patch mode
Surface;The roll body nylon cloth winding package soaked after lining system;
5)The rubber roller wrapped is put into vulcanizing tank, vulcanizing tank starts vulcanization reaction after being forced into 0.4 ~ 0.6MPa;
The process of vulcanization reaction is:
Vulcanizing tank temperature is set to rise to 100 ~ 110 DEG C in 2 ~ 2.5 hours, after heat preservation vulcanization 1 ~ 1.5 hour, then by vulcanizing tank temperature
120 ~ 135 DEG C, after heat preservation vulcanizes 1.5 ~ 2 hours are risen to, then vulcanizing tank temperature is risen to 140 ~ 150 DEG C, heat preservation vulcanization 8 ~ 10 is small
When after stop heating;Vulcanizing tank is restored to normal pressure, Temperature fall obtains fluorubber rubber roller to 50 DEG C.
On inspection, the fluorubber rubber roller tensile strength 16-18MPa that prepared by the above method, tearing strength 35-45KN/M are pulled
Disconnected elongation 300-400%, shore hardness 70-75HA, wear away 0.200 ~ 0.260cm3/1.6km。
Compared with prior art, advantage of the invention is that:
1, fluororubber formula of the invention can make linear molecule chain at solid in sulfidation in lower temperature, short time
Netted strand, product crosslink density increases after vulcanization, thus product property indices are better than universal vulcanizing system
Product.
2, the 1,4- butanediols in fluororubber formula of the invention not only improve the processing performance of fluorubber and the matter of product
Amount, while also reducing or substituting other materials, such as:The usage amount of softening agent, accelerating agent and carbon black, thus in raw material
Cost is reduced on.
Specific implementation mode
Embodiment 1
The preparation method of the fluorubber of primary low-temperature vulcanization, formula are as follows:
100 parts of crude fluororubber FE2603
15 parts of magnesia
8 parts of 1,4- butanediols
40 parts of spray carbon black
10 parts of ethyl acetate
1 part of anti-aging agent RD
2 parts of bisphenol-A;
1)Bulk portion in the fluorubber each component of primary low-temperature vulcanization is broken into powder;
2)Mixer is warming up to 120 DEG C, is put into 100 parts of fluorubber, 15 parts of magnesia, 8 parts of 1,4-butanediol and 20 parts of sprayings
Carbon black mixes 8 minutes;Remaining material is put into after mixer mixes 5 ~ 6 minutes again and obtains sizing material;
3)Sizing material is put into vulcanizing tank, starts vulcanization reaction after vulcanizing tank is forced into 0.5MP;
The process of vulcanization reaction is:
So that vulcanizing tank temperature is risen to 110 DEG C, after heat preservation vulcanizes 1 hour in 2 hours, then vulcanizing tank temperature is risen to 130 DEG C, protects
After temperature vulcanization 2 hours, then vulcanizing tank temperature risen to 145 DEG C, heat preservation vulcanization stops heating after 9 hours;By vulcanizing tank restore to
Normal pressure, Temperature fall obtain product to 50 DEG C.
On inspection, fluorubber the tensile strength 17.8MPa, tearing strength 41KN/M after above method vulcanization pull apart elongation
Rate 315%, shore hardness 74HA wear away 0.231cm3/ 1.6km, compression set rate(23℃*72h)17%.
Comparative example 1
The preparation method of the fluorubber of primary low-temperature vulcanization, formula are as follows:
100 parts of fluorubber FE2603
15 parts of magnesia
8 parts of 1,3- propylene glycol
40 parts of spray carbon black
12 parts of ethyl acetate
1 part of anti-aging agent RD
2 parts of bisphenol-A;
The preparation method is the same as that of Example 1.
On inspection, fluorubber tensile strength 14.25 MPa after above method vulcanization, tearing strength 34KN/M are pulled apart and are stretched
Long rate 346%, shore hardness 65HA wear away 0.294cm3/1.6km;Compression set rate is miscellaneous than embodiment 1 high 18.4%
Matter total content is higher than post-cure by 48.6%.
Comparative example 2
The preparation method of the fluorubber of primary low-temperature vulcanization, formula are as follows:
100 parts of fluorubber FE2603
15 parts of magnesia
8 parts of 1,4- butanediols
40 parts of spray carbon black
10 parts of Ethyl formate
1 part of anti-aging agent RD
2 parts of bisphenol-A;
The preparation method is the same as that of Example 1.
On inspection, fluorubber tensile strength 13.16 MPa after above method vulcanization, tearing strength 35KN/M are pulled apart and are stretched
Long rate 304%, shore hardness 62HA wear away 0.296cm3/1.6km;Compression set rate is miscellaneous than embodiment 1 high 22.7%
Matter total content is higher than post-cure by 61.3%.
Comparative example 3
The formula of the preparation method of the fluorubber of primary low-temperature vulcanization is formulated with embodiment 1, and method is:
1)Bulk portion in the fluorubber each component of primary low-temperature vulcanization is broken into powder;
2)Mixer is warming up to 120 DEG C, is put into 100 parts of fluorubber, 15 parts of magnesia, 8 parts of 1,4-butanediol and 20 parts of sprayings
Carbon black mixes 10 minutes;Remaining material is put into after mixer mixes 5 ~ 6 minutes again and obtains sizing material;
3)Sizing material is put into vulcanizing tank, starts vulcanization reaction after vulcanizing tank is forced into 0.5MP;
The process of vulcanization reaction is:
1. vulcanizing tank temperature is made to rise to 110 DEG C, after heat preservation vulcanizes 1 hour in 2 hours, then vulcanizing tank temperature is risen to 130 DEG C,
It keeps the temperature after vulcanizing 2 hours, then vulcanizing tank temperature is risen to 150 DEG C, heat preservation vulcanization stops heating after 10 hours;
2. vulcanizing tank is warming up to 230 DEG C of constant temperature vulcanizations for 24 hours, then by vulcanizing tank to restore to normal pressure, Temperature fall is obtained to 50 DEG C
Product.
On inspection, for the fluorubber mechanical performance after above method post-cure with embodiment 1 without significant difference, compression is permanent
Deformation rate is than embodiment 1 high 0.7%, content of impurities lower than post-cure 0.3%.
Embodiment 2
Primary low-temperature vulcanised fluororubbers are the fluorubber rubber roller of crust, by steel roll body and the vulcanization outside the roll body
Fluorubber forms.Wherein, fluorubber is grouped as by the group of following mass fraction:
100 parts of fluorubber
12 parts of magnesia
6 parts of 1,4- butanediols
35 parts of spray carbon black
8 parts of ethyl acetate
0.8 part of anti-aging agent RD
1.5 parts of bisphenol-A.
The preparation method of above-mentioned fluorubber rubber roller includes the following steps:
1)Bulk portion in each component is broken into powder;
2)Mixer is warming up to 130 DEG C, is put into fluorubber, magnesia, 1,4-butanediol and 17.5 parts of spray carbon black, is mixed
5 minutes;Remaining material is put into after mixer mixes 4 ~ 6 minutes again and obtains sizing material;
3)Sizing material is subjected to thin logical processing, 0.3 millimeter of thin slice is pressed into, then break into triangle bag, is repeated 5 times, then in mill
5-6 millimeters of film is pressed on machine, room temperature is down in ventilation, obtains fluorubber film;
4)It is special in steel roller body external coating fluorubber(Megum3290-1)Adhesive, and film is processed into adhesive tape, with squeezing
Go out or patch mode serves as a contrast system on roll body surface;The roll body nylon cloth winding package soaked after lining system;
5)The rubber roller wrapped is put into vulcanizing tank, vulcanizing tank starts vulcanization reaction after being forced into 0.6MP;
The process of vulcanization reaction is:
So that vulcanizing tank temperature is risen to 100 DEG C, after heat preservation vulcanizes 1.5 hours in 2.5 hours, then vulcanizing tank temperature is risen to 135
DEG C, it keeps the temperature after vulcanizing 1.5 hours, then vulcanizing tank temperature is risen to 140 DEG C, heat preservation vulcanization stops heating after 10 hours;It will vulcanization
Tank restores to normal pressure, and Temperature fall obtains fluorubber rubber roller to 50 DEG C.
On inspection, fluorubber the tensile strength 16.1MPa, tearing strength 42KN/M after above method vulcanization pull apart elongation
Rate 386%, shore hardness 73HA wear away 0.257cm3/1.6km.Compression set rate(23℃*72h)15%, impurity always contains
Amount is higher than 0.7% after post-cure higher than 0.6% after post-cure, compression set rate.
Embodiment 3
Primary low-temperature vulcanised fluororubbers are the fluorubber rubber roller of crust, by steel roll body and the vulcanization outside the roll body
Fluorubber forms.Wherein, fluorubber is grouped as by the group of following mass fraction:
100 parts of fluorubber FE2603
18 parts of magnesia
10 parts of 1,4- butanediols
45 parts of spray carbon black
12 parts of ethyl acetate
1.2 parts of anti-aging agent RD
2.5 parts of bisphenol-A.
The preparation method of above-mentioned fluorubber rubber roller includes the following steps:
1)Bulk portion in each component is broken into powder;
2)Mixer is warming up to 110 DEG C, is put into fluorubber, magnesia, 1,4-butanediol and 22.5 parts of spray carbon black, is mixed
10 minutes;Remaining material is put into after mixer mixes 4 ~ 6 minutes again and obtains sizing material;
3)Sizing material is subjected to thin logical processing, 0.7 millimeter of thin slice is pressed into, then break into triangle bag, is repeated 3 times, then in mill
5-6 millimeters of film is pressed on machine, room temperature is down in ventilation, obtains fluorubber film;
4)It is special in steel roller body external coating fluorubber(Megum3290-1)Adhesive, and film is processed into adhesive tape, with squeezing
Go out or patch mode serves as a contrast system on roll body surface;After lining system package is wound with the nylon cloth soaked;
5)The rubber roller wrapped is put into vulcanizing tank, vulcanizing tank starts vulcanization reaction after being forced into 0.4MP;
The process of vulcanization reaction is:
So that vulcanizing tank temperature is risen to 105 DEG C, after heat preservation vulcanizes 1.25 hours in 2.3 hours, then vulcanizing tank temperature is risen to 120
DEG C, it keeps the temperature after vulcanizing 1.75 hours, then vulcanizing tank temperature is risen to 150 DEG C, heat preservation vulcanization stops heating after 8 hours;It will vulcanization
Tank restores to normal pressure, and Temperature fall obtains fluorubber rubber roller to 50 DEG C.
On inspection, 17.5 MPa of fluorubber tensile strength after above method vulcanization, 43 KN/M of tearing strength are pulled apart and are stretched
Long rate 391%, shore hardness 75HA wear away 0.210cm3/1.6km.Compression set rate(23℃*72h)10%, it is miscellaneous
Matter total content is less than 0.4% after post-cure, and compression set rate is less than 0.2% after post-cure.
Claims (5)
1. a kind of fluorubber of primary low-temperature vulcanization, which is characterized in that be grouped as by the group of following mass fraction ratio:
100 parts of crude fluororubber
12 ~ 18 parts of magnesia
6 ~ 10 parts of 1,4- butanediols
35 ~ 45 parts of spray carbon black
8 ~ 12 parts of ethyl acetate
0.8 ~ 1.2 part of anti-aging agent RD
1.5 ~ 2.5 parts of bisphenol-A.
2. the fluorubber of primary low-temperature vulcanization according to claim 1, which is characterized in that the door of the crude fluororubber
Buddhist nun's viscosity is 50 ~ 60.
3. the preparation method for the fluorubber that primary low-temperature described in claims 1 or 2 vulcanizes, which is characterized in that including walking as follows
Suddenly:
1)Bulk portion in the fluorubber each component of primary low-temperature vulcanization is broken into powder;
2)Mixer is warming up to 110 ~ 130 DEG C, is put into crude fluororubber, magnesia, the spray of 1,4-butanediol and 1/2 formula part
Mist carbon black mixes 5 ~ 10 minutes;Remaining material is put into after mixer mixes 4 ~ 6 minutes again and obtains sizing material;
3)Sizing material is put into vulcanizing tank, starts vulcanization reaction after vulcanizing tank is forced into 0.4 ~ 0.6MPa;
The process of vulcanization reaction is:
Vulcanizing tank temperature is set to rise to 100 ~ 110 DEG C in 2 ~ 2.5 hours, after heat preservation vulcanization 1 ~ 1.5 hour, then by vulcanizing tank temperature
120 ~ 135 DEG C, after heat preservation vulcanizes 1.5 ~ 2 hours are risen to, then vulcanizing tank temperature is risen to 140 ~ 155 DEG C, heat preservation vulcanization 8 ~ 10 is small
When after stop heating;Vulcanizing tank is restored to normal pressure, Temperature fall is to 50 DEG C and hereinafter, obtains product.
4. a kind of fluorubber rubber roller, which is characterized in that claims 1 or 2 institute by steel roll body and outside the roll body
The fluorubber crust composition for the primary low-temperature vulcanization stated.
5. the preparation method of fluorubber rubber roller according to claim 4, which is characterized in that include the following steps:
1)Bulk portion in the fluorubber each component of primary low-temperature vulcanization is broken into powder;
2)Mixer is warming up to 110 ~ 130 DEG C, is put into crude fluororubber, magnesia, the spray of 1,4-butanediol and 1/2 formula part
Mist carbon black mixes 5 ~ 10 minutes;Remaining material is put into after mixer mixes 4 ~ 6 minutes again and obtains sizing material;
3)Sizing material is subjected to thin logical processing, is pressed into 0.3 ~ 0.7 millimeter of thin slice, then break into triangle bag, repetition 3 ~ 5 times, then
It is pressed into 5-6 millimeters of film on a mill, room temperature is down in ventilation, obtains fluorubber film;
4)In steel roller body surface face brushing adhesive, and film is processed into adhesive tape, system is served as a contrast in roll body with extrusion or patch mode
Surface;The roll body nylon cloth winding package soaked after lining system;
5)The rubber roller wrapped is put into vulcanizing tank, vulcanizing tank starts vulcanization reaction after being forced into 0.4 ~ 0.6MPa;
The process of vulcanization reaction is:
Vulcanizing tank temperature is set to rise to 100 ~ 110 DEG C in 2 ~ 2.5 hours, after heat preservation vulcanization 1 ~ 1.5 hour, then by vulcanizing tank temperature
120 ~ 135 DEG C, after heat preservation vulcanizes 1.5 ~ 2 hours are risen to, then vulcanizing tank temperature is risen to 140 ~ 150 DEG C, heat preservation vulcanization 8 ~ 10 is small
When after stop heating;Vulcanizing tank is restored to normal pressure, Temperature fall obtains fluorubber rubber roller to 50 DEG C.
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CN106317713A (en) * | 2016-08-31 | 2017-01-11 | 南京利德东方橡塑科技有限公司 | Abrasion-resistant high-temperature-resistant tear-resistant fluorine rubber and preparation method thereof |
CN107434896A (en) * | 2017-08-29 | 2017-12-05 | 高科橡塑工业有限公司 | It is molded seamless vulcanizable fluororubber adhesive tape and preparation method thereof |
CN108003400A (en) * | 2017-12-11 | 2018-05-08 | 上海双浦橡胶防腐衬里有限公司 | A kind of high-temperature resistant rubber liner compositions and its preparation method and application |
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